Search results for: microstructure analysis

Authors: S. Nqayi

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Understanding the structural, electronic, and magnetic properties of nanomaterials is essential for developing next-generation electronic and spintronic devices, contributing to the progress of nanoscience and nanotechnology applications. Multiferroic materials, with intimately coupled ferroic-order parameters, are widely considered to breed fascinating physical properties and provide unique opportunities for the development of next-generation devices, like multistate non-volatile memory. In this study, we are set to investigate the structural, electronic, and magnetic properties of the frustrated Feᴵᴵ/Smⱽᴵ sublattice in relation to the widely studied perovskites for spintronics applications. The atomic composition, microstructure, crystallography, magnetization, thermal, and dielectric properties of a pyrochlore Sm₂Fe₂O₇ system synthesized using sol-gel methods are currently being investigated. Precursor powders were dissolved in citric acid monohydrate to obtain a solution. The obtained solution was stirred and heated using a magnetic stirrer to obtain the gel phase. Then, the gel was dried at 200°C to remove water and organic compounds and form an orange powder. The X-ray diffraction analysis confirms that the structure crystallized as a pyrochlore structure with a tetragonal F4mm (107) symmetry. The presence of Fe³⁺/Fe⁴⁺ mixed states is also revealed by XPS analysis.

Keywords: nanostructures, multiferroic materials, pyrochlores, spintronics

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Authors: JongWon Han, NoHoon Kim, HyoIk Ahn, HaeWoo Lee

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In this study, shielded metal arc welding was performed as a function of Nb content at 2.24 wt%, 3.25 wt%, and 4.26 wt%. The microstructure was observed using scanning electron microscopy/energy dispersive X-ray spectroscopy (SEM/EDS) and showed the development of a columnar dendrite structure in the specimen having the least Nb content. From the hardness test, the hardness value was confirmed to reduce with decreasing Nb content. From electron backscatter diffraction (EBSD) analysis, the largest grain size was found in the specimen with Nb content of 2.24 wt%. The potentiodynamic polarization test was carried out to determine the pitting corrosion resistance; there was no significant difference in the pitting corrosion resistance with increasing Nb content. To evaluate the degree of sensitization to intergranular corrosion, the Double Loop Electrochemical Potentiodynamic Reactivation(DL-EPR test) was conducted. A similar degree of sensitization was found in two specimens except with a Nb content of 2.24 wt%, while a relatively high degree of sensitization was found in the specimen with a Nb content of 2.24 wt%.

Keywords: inconel 625, Nb content, potentiodynamic test, DL-EPR test

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Authors: Liliana Zura-Brravo, Antonio Vega-Galvez, Roberto Lemus-Mondaca, Jessica Lopez

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Murta (Ugni molinae T.) is an endemic fruit of Southern Chile, possesses qualities exceptional as its high antioxidants content, that make it increasingly more appreciated for marketing. Dehydration has the potential providing safe food products through the decreased activity water while maintaining their functional properties. The objective of this study was to evaluate the effect of different drying methods on the antioxidant capacity (AC), total flavonoid content (TFC), rehydration indexes and texture the dried murta berry. Five drying technologies were used: convective drying, vacuum drying, sun-air drying, infrared drying and freezing-drying. The antioxidant capacity was measured by the ORAC method, CFT was determined by spectrophotometry, rehydration capacity (CR) and water retention (WHC) by gravimetry, texture profile (TPA) by a texture analyzer TA-XT2 and microstructure by SEM. The results showed that the lyophilized murta had smaller losses AC and TFC with values of 2886.27 routine mg rutin/ 100 g dm and 23359.99 μmol ET/100 g dm, respectively. According to the rehydration indexes, these were affected by the drying methods, where the maximum value of WHC was 92.60 g retained water/100 g sample for the vacuum drying, and the lowest value of CR was 1.43 g water absorbed/g dm for the sun-air drying. Furthermore, the microstructure and TPA showed that lyophilized samples had characteristics similar to the fresh sample. Therefore, it is possible to mention that lyophilization achieved greater extent preserving the characteristics of the murta samples, showing that this method can be used in the food industry and encourage the consumption of dried fruit and thus give it greater added value.

Keywords: antioxidant, drying method, flavonoid, murta berry, texture

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Authors: Helen S. Joyner (Melito), Mohammad Anvari

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Concentrated emulsions stabilized by proteins are systems of great importance in food, pharmaceutical and cosmetic products. Controlling emulsion rheology is critical for ensuring desired properties during formation, storage, and consumption of emulsion-based products. Studies on concentrated emulsions have focused on rheology of monodispersed systems. However, emulsions used for industrial applications are polydispersed in nature, and this polydispersity is regarded as an important parameter that also governs the rheology of the concentrated emulsions. Therefore, the objective of this study was to characterize rheological (small and large deformation behaviors) and microstructural properties of concentrated emulsions which were not truly monodispersed as usually encountered in food products such as margarines, mayonnaise, creams, spreads, and etc. The concentrated emulsions were prepared at different concentrations of fish gelatin (0.2, 0.4, 0.8% w/v in the whole emulsion system), oil-water ratio 80-20 (w/w), homogenization speed 10000 rpm, and 25oC. Confocal laser scanning microscopy (CLSM) was used to determine the microstructure of the emulsions. To prepare samples for CLSM analysis, FG solutions were stained by Fluorescein isothiocyanate dye. Emulsion viscosity profiles were determined using shear rate sweeps (0.01 to 100 1/s). The linear viscoelastic regions (LVRs) of the emulsions were determined using strain sweeps (0.01 to 100% strain) for each sample. Frequency sweeps were performed in the LVR (0.1% strain) from 0.6 to 100 rad/s. Large amplitude oscillatory shear (LAOS) testing was conducted by collecting raw waveform data at 0.05, 1, 10, and 100% strain at 4 different frequencies (0.5, 1, 10, and 100 rad/s). All measurements were performed in triplicate at 25oC. The CLSM results revealed that increased fish gelatin concentration resulted in more stable oil-in-water emulsions with homogeneous, finely dispersed oil droplets. Furthermore, the protein concentration had a significant effect on emulsion rheological properties. Apparent viscosity and dynamic moduli at small deformations increased with increasing fish gelatin concentration. These results were related to increased inter-droplet network connections caused by increased fish gelatin adsorption at the surface of oil droplets. Nevertheless, all samples showed shear-thinning and weak gel behaviors over shear rate and frequency sweeps, respectively. Lissajous plots, or plots of stress versus strain, and phase lag values were used to determine nonlinear behavior of the emulsions in LAOS testing. Greater distortion in the elliptical shape of the plots followed by higher phase lag values was observed at large strains and frequencies in all samples, indicating increased nonlinear behavior. Shifts from elastic-dominated to viscous dominated behavior were also observed. These shifts were attributed to damage to the sample microstructure (e.g. gel network disruption), which would lead to viscous-type behaviors such as permanent deformation and flow. Unlike the small deformation results, the LAOS behavior of the concentrated emulsions was not dependent on fish gelatin concentration. Systems with different microstructures showed similar nonlinear viscoelastic behaviors. The results of this study provided valuable information that can be used to incorporate concentrated emulsions in emulsion-based food formulations.

Keywords: concentrated emulsion, fish gelatin, microstructure, rheology

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Authors: M. Riazat, H. Abdolvand, M. Baniassadi

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In this present work, 3D reconstruction of cathode of SOFC is developed with various volume fractions and porosity. Three Phase Boundary (TPB) of construction of such derived micro structures is calculated. The neural network is used to optimize the porosity and volume fraction of each phase to reach a structure with maximum TPB.

Keywords: fuel cell, solid oxide, TPB, 3D reconstruction

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Authors: Souvik Das, Janak Lal, Arthita Dey, Goutam Mukhopadhyay, Sandip Bhattacharya

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Telescopic Front Fork (TFF) used in two wheelers, mainly motorcycle, is made from high strength steel, and is manufactured by high frequency induction welding process wherein hot rolled and pickled coils are used as input raw material for rolling of hollow tubes followed by heat treatment, surface treatment, cold drawing, tempering, etc. The final application demands superior quality TFF tubes w.r.t. surface finish and dimensional tolerances. This paper presents the investigation of two different types of failure of fork during operation. The investigation consists of visual inspection, chemical analysis, characterization of microstructure, and energy dispersive spectroscopy. In this paper, comprehensive investigations of two failed tube samples were investigated. In case of Sample #1, the result revealed that there was a pre-existing crack, known as hook crack, which leads to the cracking of the tube. Metallographic examination exhibited that during field operation the pre-existing hook crack was surfaced out leading to crack in the pipe. In case of Sample #2, presence of internal oxidation with decarburised grains inside the material indicates origin of the defect from slab stage.

Keywords: telescopic front fork, induction welding, hook crack, internal oxidation

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Authors: G. Singh, H.Schuster, U. Füssel

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The stability of electric arc and durability of electrode tip used in Tungsten Inert Gas (TIG) welding demand a metallurgical study about the chemical transport mechanism of emitter oxide particles in tungsten electrode during its real welding conditions. The tungsten electrodes doped with emitter oxides of rare earth oxides such as La₂O₃, Th₂O₃, Y₂O₃, CeO₂ and ZrO₂ feature a comparatively lower work function than tungsten and thus have superior emission characteristics due to lesser surface temperature of the cathode. The local change in concentration of these emitter particles in tungsten electrode due to high temperature diffusion (chemical transport) can change its functional properties like electrode temperature, work function, electron emission, and stability of the electrode tip shape. The resulting increment in tip surface temperature results in the electrode material loss. It was also observed that the tungsten recrystallizes to large grains at high temperature. When the shape of grain boundaries are granular in shape, the intergranular diffusion of oxide emitter particles takes more time to reach the electrode surface. In the experimental work, the microstructure of the used electrode's tip surface will be studied by scanning electron microscope and reflective X-ray technique in order to gauge the extent of the diffusion and chemical reaction of emitter particles. Besides, a simulated model is proposed to explain the effect of oxide particles diffusion on the electrode’s microstructure, electron emission characteristics, and electrode tip erosion. This model suggests metallurgical modifications in tungsten electrode to enhance its erosion resistance.

Keywords: rare-earth emitter particles, temperature-dependent diffusion, TIG welding, Tungsten electrode

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Authors: M. I. Equbal, R. K. Ohdar, B. Singh, P. Talukdar

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Micro-alloyed steel components are used in automotive industry for the necessity to make the manufacturing process cycles shorter when compared to conventional steel by eliminating heat treatment cycles, so an important saving of costs and energy can be reached by reducing the number of operations. Micro-alloying elements like vanadium, niobium or titanium have been added to medium carbon steels to achieve grain refinement with or without precipitation strengthening along with uniform microstructure throughout the matrix. Present study reports the applicability of medium carbon vanadium micro-alloyed steel in hot forging. Forgeability has been determined with respect to different cooling rates, after forging in a hydraulic press at 50% diameter reduction in temperature range of 900-11000C. Final microstructures, hardness, tensile strength, and impact strength have been evaluated. The friction coefficients of different lubricating conditions, viz., graphite in hydraulic oil, graphite in furnace oil, DF 150 (Graphite, Water-Based) die lubricant and dry or without any lubrication were obtained from the ring compression test for the above micro-alloyed steel. Results of ring compression tests indicate that graphite in hydraulic oil lubricant is preferred for free forging and dry lubricant is preferred for die forging operation. Exceptionally good forgeability and high resistance to fracture, especially for faster cooling rate has been observed for fine equiaxed ferrite-pearlite grains, some amount of bainite and fine precipitates of vanadium carbides and carbonitrides. The results indicated that the cooling rate has a remarkable effect on the microstructure and mechanical properties at room temperature.

Keywords: cooling rate, hot forging, micro-alloyed, ring compression

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Authors: Kaushal Kishore, Vaibhav Jain, Hrishikesh Jugade, Saurabh Hadas, Manashi Adhikary, Goutam Mukhopadhyay, Sandip Bhattacharyya

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Rotary air compressors in air conditioners are used to suck excessive volume of air from the atmosphere in a small space to provide drive to the components attached to them. Hydraulic test is one of the most important methods to decide the suitability of these components for usage. In the present application, projection welding is used to join the hot rolled steel sheets after forming for manufacturing of air compressors. These sheets belong to two different high strength low alloy (HSLA) steel grades. It was observed that one batch of compressors made of a particular grade was cracking from the weld, whereas those made of another grade were passing the hydraulic tests. Cracking was repeatedly observed from the weld location. A detailed comparative study of the compressors which failed and successfully passed pressure tests has been presented. Location of crack initiation was identified to be the interface of fusion zone/heat affected zone. Shear dimples were observed on the fracture surface confirming the ductile mode of failure. Hardness profile across the weld revealed a sharp rise in hardness in the fusion zone. This was attributed to the presence of untempered martensitic lath in the fusion zone. A sharp metallurgical notch existed at the heat affected zone/fusion zone interface due to transition in microstructure from acicular ferrite and bainite in HAZ to untempered martensite in the fusion zone. In contrast, welds which did not fail during the pressure tests showed a smooth hardness profile with no abnormal rise in hardness in the fusion zone. The bainitic microstructure was observed in the fusion zone of successful welds. This difference in microstructural constituents in the fusion zone was attributed to the presence of a small amount of boron (0.002 wt. %) in the sheets which were cracking. Trace amount of boron is known to substantially increase the hardenability of HSLA steel, and cooling rate during resolidification in the fusion zone is sufficient to form martensite. Post-weld heat treatment was recommended to transform untempered martensite to tempered martensite with lower hardness.

Keywords: compressor, cracking, martensite, weld, boron, hardenability, high strength low alloy steel

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Authors: Aakanchha Jain, D. V. Kohli

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Cubosomes are nanoparticles but instead of the solid particles, cubosomes are self-assembled liquid crystalline particles of certain surfactant with proper ratio of water with a microstructure that provides unique properties of practical interest. Cubosomes encapsulating Fluconazole were prepared by emulsification method and characterized for particle size, entrapment efficiency. The cubosomes prepared were 257.2±2.94 nm in size with drug entrapment efficiency of 66.2±2.69%. The optimized formulation characterized for shape and surface morphology by TEM and SEM analysis. SEM photograph showed the smooth surface of optimized cubosomes and TEM photograph revealed square somewhat circular intact shapes of cubosomes. MIC was determined by XTT based method and antifungal activity was determined in vitro. The cumulative percentage of Fnz from cubosomes permeated via dialysis membrane (MWCO 12-14 KD) showed a percent cumulative drug release of 76.86% while Fnz solution showed release up to 91.04% in 24 hours in PBS (pH 6.5)(p < 0.005).

Keywords: Candids albicans, cubosomes, fluconazole, topical delivery

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Authors: P. Jayaram, Prasoon Prasannan, N. K. Deepak, P. P. Pradyumnan

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Indium and Zirconium co doped zinc oxide (InZrZnO) thin films are prepared by chemical spray pyrolysis method on pre-heated quartz substrates. The films are subjected to vacuum annealing at 400ᵒC for three hours in an appropriate air (10-5mbar) ambience after deposition. X-ray diffraction, Scanning electron microscopy, energy dispersive spectra and photoluminescence are used to characterize the films. Temperature dependent electrical measurements are conducted on the films and the films exhibit exceptional conductivity at higher temperatures. XRD analysis shows that all the films prepared in this work have hexagonal wurtzite structure. The average crystallite sizes of the films were calculated using Scherrer’s formula, and uniform deformation model (UDM) of Williamson-Hall method is used to establish the micro-strain values. The dislocation density is determined from the Williamson and Smallman’s formula. Intense, broad and strongly coupled multiple photoluminescence were observed from photoluminescence spectra. PL indicated relatively high concentration defective oxygen and Zn vacancies in the film composition. Strongly coupled ultraviolet near blue emissions authenticate that the dopants are capable of inducing modulated free excitonic (FX), donor accepter pair (DAP) and longitudinal optical phonon emissions in thin films.

Keywords: PL, SEM, TCOs, thin films, XRD

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Authors: S. Gupta, R. Sarkar, S. Pathak, D. H. Kela, A. Pramanick, P. Talukdar

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Low alloy quenched and tempered steels are typically used in cast railway components such as knuckles, yokes, and couplers. Since these components experience extensive impact loading during their service life, adequate impact toughness of these grades need to be ensured to avoid catastrophic failure of parts in service. Because of the general availability of Charpy V Test equipment, Charpy test is the most common and economical means to evaluate the impact toughness of materials and is generally used in quality control applications. With this backdrop, an experiment was designed to evaluate the effect of austenitizing temperature, soaking time and resultant grain size on the Charpy impact toughness and the related fracture mechanisms in a quenched and tempered low alloy steel, with the aim of optimizing the heat treatment parameters (i.e. austenitizing temperature and soaking time) with respect to impact toughness. In the first phase, samples were austenitized at different temperatures viz. 760, 800, 840, 880, 920 and 960°C, followed by quenching and tempering at 600°C for 4 hours. In the next phase, samples were subjected to different soaking times (0, 2, 4 and 6 hours) at a fixed austenitizing temperature (980°C), followed by quenching and tempering at 600°C for 4 hours. The samples corresponding to different test conditions were then subjected to instrumented Charpy tests at -40°C and energy absorbed were recorded. Subsequently, microstructure and fracture surface of samples corresponding to different test conditions were observed under scanning electron microscope, and the corresponding grain sizes were measured. In the final stage, austenitizing temperature, soaking time and measured grain sizes were correlated with impact toughness and the fracture morphology and mechanism.

Keywords: heat treatment, grain size, microstructure, retained austenite and impact toughness

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Authors: T. Deepa, S. R. Inchara, S. V. Venkatesh, Seema Tharannum

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Concrete is the most widely used structural material. It is made using locally available materials. However, Concrete has low tensile strength and may crack in the early days with exothermic hydration. Bacillus subtilis bacteria that form endospores is the biological agent considered in this study for Biomineralization or MICP (Microbially Induced Calcite Precipitation) Technique and to address the increased Construction water demand, Recycled Grey Water which is obtained from STP of PES University, opted in place of Potable water. In this work, M30 grade conventional concrete is designed using OPC 53 grade cement, Manufactured Sand, Natural coarse aggregates, and Potable water. Conventional Concrete (CC), Bacterial Concrete with Potable water (BS), and Recycled Grey Water concrete (RGW) are the three different concrete specimens casted. Experimental studies such as the strength test and the surface hardness test are conducted on Conventional and Bacterial concrete samples after 7, 28, and 56 days of curing. Concrete cubes are subjected to a temperature of 50° C to investigate the effect of higher temperature. Cracked cube specimens are observed for Self-healing - as well as microstructure analysis with Scanning Electron Microscope (SEM), Energy Dispersive X-Ray Analysis (EDAX), and X-Ray Diffraction Analysis (XRD).Noticeable Calcium salt deposition is observed on the surface of BS and RGW cracked specimen. Surface hardness and EDAX test gave promising result on the advantage of using spore-forming bacteria in concrete. This is followed by the strength gain in Compression and Flexure. Results also indicate that Recycled Grey Water can be a substitute for Normal water in concrete.

Keywords: bacillus subtilis, bacterial concrete, recycled grey water, self-healing, surface hardness of concrete

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Authors: Soumyajit Koley, Kuladeep Rajamudili, Supriyo Ganguly

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In recent years, iron-based shape-memory alloys have been emerging as an inexpensive alternative to costly Ni-Ti alloy and thus considered suitable for many different applications in civil structures. Fe-17Mn-10Cr-5Si-4Ni-0.5V-0.5C alloy contains 37 wt.% of total solute elements. Such complex multi-component metallurgical system often leads to severe solute segregation and solidification cracking. Wire-arc additive manufacturing (WAAM) of Fe-17Mn-10Cr-5Si-4Ni-0.5V-0.5C alloy was attempted using a cold-wire fed plasma arc torch attached to a 6-axis robot. Self-standing walls were manufactured. However, multiple vertical cracks were observed after deposition of around 15 layers. Microstructural characterization revealed open surfaces of dendrites inside the crack, confirming these cracks as solidification cracks. Machine hammer peening (MHP) process was adopted on each layer to cold work the newly deposited alloy. Effect of MHP traverse speed were varied systematically to attain a window of operation where cracking was completely stopped. Microstructural and textural analysis were carried out further to correlate the peening process to microstructure.MHP helped in many ways. Firstly, a compressive residual stress was induced on each layer which countered the tensile residual stress evolved from solidification process; thus, reducing net tensile stress on the wall along its length. Secondly, significant local plastic deformation from MHP followed by the thermal cycle induced by deposition of next layer resulted into a recovered and recrystallized equiaxed microstructure instead of long columnar grains along the vertical direction. This microstructural change increased the total crack propagation length and thus, the overall toughness. Thirdly, the inter-layer peening significantly reduced the strong cubic {001} crystallographic texture formed along the build direction. Cubic {001} texture promotes easy separation of planes and easy crack propagation. Thus reduction of cubic texture alleviates the chance of cracking.

Keywords: Iron-based shape-memory alloy, wire-arc additive manufacturing, solidification cracking, inter-layer cold working, machine hammer peening

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Authors: Altoumi Alndalusi

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The work examines the aqueous corrosion behavior of grades of stain less steel which are used as corrosion resistant castings for applications such as valve and pump bodies. The corrosion behavior of steels in the as-cast condition has been examined using potentiostatic studies to illustrate the need for correct thermal treatment. A metallurgical examination and chemical analysis were carried out to establish the morphology of the steel structure. Heat treatment was carried out in order to compare damage in relation to microstructure. Optical and scanning electron microscopy examinations confirmed that the austenitic steels suffers from severe localized inter-dendritic pitting attack, while non homogenized castings highly alloyed duplex steels gave inferior corrosion resistance. Through the heat treatment conditions a significant of phase transformation of the duplex steel C were occurred (from ferrite to austenite and sigma plus carbides) and were gave reduction resistance.

Keywords: cast, corrosion, duplex stainless, heat treatment, material, steel

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Authors: M. N. Baig, F. N. Khan, M. Junaid

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Titanium alloys are widely employed in aerospace, medical, chemical, and marine applications. These alloys offer many advantages such as low specific weight, high strength to weight ratio, excellent corrosion resistance, high melting point and good fatigue behavior. These attractive properties make titanium alloys very unique and therefore they require special attention in all areas of processing, especially welding. In this work, 1.6 mm thick sheets of Ti-5Al-2,5Sn, an alpha titanium (α-Ti) alloy, were welded using electron beam (EBW) and laser beam (LBW) welding processes to achieve a full penetration Bead-on Plate (BoP) configuration. The weldments were studied using polarized optical microscope, SEM, EDS and XRD. Microhardness distribution across the weld zone and smooth and notch tensile strengths of the weldments were also recorded. Residual stresses using Hole-drill Strain Measurement (HDSM) method and deformation patterns of the weldments were measured for the purpose of comparison of the two welding processes. Fusion zone widths of both EBW and LBW weldments were found to be approximately equivalent owing to fairly similar high power densities of both the processes. Relatively less oxide content and consequently high joint quality were achieved in EBW weldment as compared to LBW due to vacuum environment and absence of any shielding gas. However, an increase in heat-affected zone width and partial ά-martensitic transformation infusion zone of EBW weldment were observed because of lesser cooling rates associated with EBW as compared with LBW. The microstructure infusion zone of EBW weldment comprised both acicular α and ά martensite within the prior β grains whereas complete ά martensitic transformation was observed within the fusion zone of LBW weldment. Hardness of the fusion zone in EBW weldment was found to be lower than the fusion zone of LBW weldment due to the observed microstructural differences. Notch tensile specimen of LBW exhibited higher load capacity, ductility, and absorbed energy as compared with EBW specimen due to the presence of high strength ά martensitic phase. It was observed that the sheet deformation and deformation angle in EBW weldment were more than LBW weldment due to relatively more heat retention in EBW which led to more thermal strains and hence higher deformations and deformation angle. The lowest residual stresses were found in LBW weldments which were tensile in nature. This was owing to high power density and higher cooling rates associated with LBW process. EBW weldment exhibited highest compressive residual stresses due to which the service life of EBW weldment is expected to improve.

Keywords: Laser and electron beam welding, Microstructure and mechanical properties, Residual stress and distortions, Titanium alloys

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Authors: Sasan Talebnezhad, Saeed Pormahdian, Naghi Assali

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Homogeneous α-diimine nickel (II) catalyst complexes, with and without amino para-aryl position functionality, were synthesized. These complexes were immobilized on carboxyl, hydroxyl, and acyl chloride functionalized multi-walled carbon nanotubes to form five novel heterogeneous α-diiminonickel catalysts. Immobilization was performed by covalent or electrostatic bonding via methylaluminoxane (MAO) linker or amide linkage. Both the nature of α-diimine ligands and the kind of interaction between anchored catalyst complexes and multi-walled carbon nanotube surface influenced the catalytic performance, microstructure, and morphology of obtained polyethylenes. The catalyst prepared by amide bonding showed lowest relative weight loss in thermogravimetry analysis and highest activities up to 5863 gr PE mmol-1Ni.hr-1. This catalyst produced polyethylene with dense botryoidal morphology.

Keywords: α-diimine nickel (II) complexes, immobilization, multi-walled carbon nanotubes, ethylene polymerization

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Authors: Sasan Talebnezhad, Saeed Pourmahdian, Naghi Assali

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Homogeneous α-diimine nickel (II) catalyst complexes, with and without amino para-aryl position functionality, were synthesized. These complexes were immobilized on carboxyl, hydroxyl and acyl chloride functionalized multi-walled carbon nanotubes to form five novel heterogeneous α diiminonickel catalysts. Immobilization was performed by covalent or electrostatic bonding via methylaluminoxane (MAO) linker or amide linkage. Both the nature of α-diimine ligands and the kind of interaction between anchored catalyst complexes and multi-walled carbon nanotube surface influenced the catalytic performance, microstructure, and morphology of obtained polyethylenes. The catalyst prepared by amide bonding showed lowest relative weight loss in thermogravimetry analysis and highest activities up to 5863 gr PE mmol-1Ni.hr-1. This catalyst produced polyethylene with dense botryoidal morphology.

Keywords: α-diimine nickel (II) complexes, immobilization, multi-walled carbon nanotubes, ethylene polymerization

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Authors: Suhaib Salahuddin Alzubair Suliman

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This paper examines the mechanical strength of different binders including pure ordinary Portland cement (OPC) and others having OPC supplemented by two maximum sizes of waste glass powder (GP) of 75-μm and 150μm. Chemical analysis of the GPs using PCEDX test analysis has revealed it silica (SiO2 ) content % is 86.883 and Calcium oxide (CaO) is 12.203%while there are traces of other impurities . Furthermore, the specific gravity of GP was measured. The experiments have been conducted on 63 specimens mortar made with standard sand with 20%,25%, and 30% of GP levels of substituting OPC. The specimens are tested at 3, 7 and 28 days for compressive strength and flexural strength. The specimens made with maximum GP size of 75-μm have outperformed the control OPC mortar at 28 days test age than size 150-μm at various replacement levels. In addition to that, the mechanical strengths were evaluated compressive strength and flexural strength tests were conducted for GPs. The findings from this study indicated that the mortars modified with GP 75μm and replacement ratio of 20% showed an improvement in compressive strength and flexural strength compared to the control mortar at the 28 days of curing with significant development between 7 and 28 days. Mortar with GP size 75-μm containing 30% & 20% replacement of cement have exhibited the highest flexural strength among all mortar mixtures. The improvement in the mechanical strength of the mortars modified with GP can be attributed to the pozzolanic property of GPs, which leads to a more densified microstructure and improved interfacial bonding between sand and cement paste matrix in mortars.

Keywords: glass powder, pozzolana, compressive strength, flexural strength, mortar

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Authors: Yonosuke Murayama

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We have developed and studied a metastable beta Ti alloy, which shows super-elasticity and low Young’s modulus according to the phase stability of its beta phase. The super-elasticity and low Young’s modulus are required in a wide range of applications in various industrial fields. For example, the metallic implant with low Young’s modulus and non-toxicity is desirable because the large difference of Young’s modulus between the human bone and the implant material may cause a stress-shielding phenomenon. We have investigated the role of Sn and Al in metastable beta Ti-Cr-Sn, Ti-Cr-Al, Ti-V-Sn, and Ti-V-Al alloys. The metastable beta Ti-Cr-Sn, Ti-Cr-Al, Ti-V-Sn, and Ti-V-Al alloys form during quenching from the beta field at high temperature. While Cr and V act as beta stabilizers, Sn and Al are considered as elements to suppress the athermal omega phase produced during quenching. The athermal omega phase degrades the properties of super-elasticity and Young’s modulus. Although Al and Sn as single elements are considered as an alpha stabilizer and neutral, respectively, Sn and Al acted also as beta stabilizers when added simultaneously with beta stabilized element of Cr or V in this experiment. The quenched microstructure of Ti-Cr-Sn, Ti-Cr-Al, Ti-V-Sn, and Ti-V-Al alloys shifts from martensitic structure to beta single-phase structure with increasing Cr or V. The Young’s modulus of Ti-Cr-Sn, Ti-Cr-Al, Ti-V-Sn, and Ti-V-Al alloys decreased and then increased with increasing Cr or V, each showing its own minimum value of Young's modulus respectively. The composition of the alloy with the minimum Young’s modulus is a near border composition where the quenched microstructure shifts from martensite to beta. The border composition of Ti-Cr-Sn and Ti-V-Sn alloys required only less amount of each beta stabilizer, Cr or V, than Ti-Cr-Al and Ti-V-Al alloys. This indicates that the effect of Sn as a beta stabilizer is stronger than Al. Sn and Al influenced the competitive relation between stress-induced martensitic transformation and slip deformation. Thus, super-elastic properties of metastable beta Ti-Cr-Sn, Ti-Cr-Al, Ti-V-Sn, and Ti-V-Al alloys varied depending on the alloyed element, Sn or Al.

Keywords: metastable beta Ti alloy, super-elasticity, low Young’s modulus, stress-induced martensitic transformation, beta stabilized element

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Authors: Nisrin R. Abdelal, Steven L. Donaldson

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Composite materials are widely used in aviation industry due to their superior properties; however, they are susceptible to delamination. Through-thickness stitching is one of the techniques to alleviate delamination. Kevlar is one of the most common stitching materials; in contrast, it is expensive and presents stitching fabrication challenges. Therefore, this study compares the performance of Kevlar with an inexpensive and easy-to-use nylon fiber in stitching to alleviate delamination. Three laminates of unidirectional carbon fiber-epoxy composites were manufactured using vacuum assisted resin transfer molding process. One panel was stitched with Kevlar, one with nylon, and one unstitched. Mode I interlaminar fracture tests were carried out on specimens from the three composite laminates, and the results were compared. Fractographic analysis using optical and scanning electron microscope were conducted to reveal the differences between stitching with Kevlar and nylon on the internal microstructure of the composite with respect to the interlaminar fracture toughness values.

Keywords: carbon, delamination, Kevlar, mode I, nylon, stitching

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Authors: M. Arunachalam, M. Pandey

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Nacre, a biological material that forms the inner-layer of sea shells can achieve high toughness and strength by way of staggered arrangement of strong tablets with soft and weak organic interface. Under applied loads the tablets slide over the adjacent tablets, thus generating inelastic deformation and toughness on macroscopic scale. A two dimensional finite element based homogenization methodology is adopted for obtaining the effective material properties of Nacre using a representative volume element (RVE) at finite deformations. In this work, the material behaviour for tablet and interface are assumed to be Isotropic elastic and Isotropic elastic-perfectly plastic with strain softening respectively. Numerical experiments such as uniaxial tension test along X, Y directions and simple shear test are performed on the RVE with uniform displacement and periodic constraints applied at the RVE boundaries to obtain the anisotropic homogenized response and maximum local stresses within each constituents of Nacre. Homogenized material model is then tested for macroscopic structure under three point bending condition and the results obtained are comparable with the results obtained for detailed microstructure based structure, thus homogenization provides a bridge between macroscopic scale and microscopic scale and homogenized material properties obtained from microstructural (RVE) analysis could be used in large scale structural analysis.

Keywords: finite element, homogenization, inelastic deformation, staggered arrangement

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Authors: Venkatesan Sundaramoorthy

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The field of ceramics has undergone a remarkable transformation with the advent of additive manufacturing technologies. This comprehensive review explores the mechanical properties of additively manufactured ceramic components, focusing on key materials such as Alumina, Zirconia, and Silicon Carbide. The study delves into various authors' review technology into the various additive manufacturing techniques, including Stereolithography, Powder Bed Fusion, and Binder Jetting, highlighting their advantages and challenges. It provides a detailed analysis of the mechanical properties of these ceramics, offering insights into their hardness, strength, fracture toughness, and thermal conductivity. Factors affecting mechanical properties, such as microstructure and post-processing, are thoroughly examined. Recent advancements and future directions in 3D-printed ceramics are discussed, showcasing the potential for further optimization and innovation. This review underscores the profound implications of additive manufacturing for ceramics in industries such as aerospace, healthcare, and electronics, ushering in a new era of engineering and design possibilities for ceramic components.

Keywords: mechanical properties, additive manufacturing, ceramic materials, PBF

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Authors: Chia-Chia Chang, Jhen-Ting Huang, Hu-Cheng Weng, An-Ya Lo

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This study developed a simple hierarchical porous carbon (HPC) synthesis process and used for supercapacitor application. In which, mesopore provides huge specific surface area, meanwhile, macropore provides excellent mass transfer. Thus the hierarchical porous electrode improves the charge-discharge performance. On the other hand, cerium oxide (CeO2) have also got a lot research attention owing to its rich in content, low in price, environmentally friendly, good catalytic properties, and easy preparation. Besides, a rapid redox reaction occurs between trivalent cerium and tetravalent cerium releases oxygen atom and increase the conductivity. In order to prevent CeO2 from disintegration under long-term charge-discharge operation, the CeO2 carbon porous materials were was integrated as composite material in this study. For in the ex-situ analysis, scanning electron microscope (SEM), X-ray diffraction (XRD), transmission electron microscope (TEM) analysis were adopted to identify the surface morphology, crystal structure, and microstructure of the composite. 77K Nitrogen adsorption-desorption analysis was used to analyze the porosity of each specimen. For the in-situ test, cyclic voltammetry (CV) and chronopotentiometry (CP) were conducted by potentiostat to understand the charge and discharge properties. Ragone plot was drawn to further analyze the resistance properties. Based on above analyses, the effect of macropores/mespores and the CeO2/HPC ratios on charge-discharge performance were investigated. As a result, the capacitance can be greatly enhanced by 2.6 times higher than pristine mesoporous carbon electrode.

Keywords: hierarchical porous carbon, cerium oxide, supercapacitor

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Authors: Kumar Sankaran, Santanu Chattopadhyay, Golok Behari Nando, Sujith Nair, Sreejesh Arayambath, Unnikrishnan Govindan

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Rubber nanocomposites based on Bromobutyl rubber (BIIR), Polyepichlorohydrin rubber (CO), Carbon black (CB) and organically modified montmorillonite clay (NC) were prepared via melt compounding technique. The developed quaternary nanocomposites were characterized analytically and their properties were compared against the standard BIIR compound. BIIR-CO nanocomposites showed improved physico-mechanical properties as compared to that of the standard BIIR compound. Hybrid microstructure (NC-CB) development, clay exfoliation and better filler dispersion in the quaternary nanocomposite significantly contributed to the overall enhancement of properties. Introduction of CO in the system increased the specific gravity and hardness of the compound as compared to that of the standard compound. XRD analysis, AFM imaging and HR-TEM measurements confirmed exfoliation and a good level of dispersion of the NC in the composites. Permeability of developed BIIR-CO nanocomposites decreases significantly as compared to that of the standard BIIR compound.

Keywords: rubber nanocomposites, morphology, permeability, BIIR

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Authors: Jae-Ho Jang, Jung-Soo Kim, Byung-Jun Kim, Dae-Geun Nam, Uoo-Chang Jung, Yoon-Suk Choi

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Low alloy steels are widely used for pressure vessels, spent fuel storage, and steam generators required to withstand the internal pressure and prevent unexpected failure in nuclear power plants, which these may suffer embrittlement by high levels of radiation and heat for a long period. Therefore, it is important to improve mechanical properties of low alloy steels for the integrity of structure materials at an early stage of fabrication. Recently, it showed that a double austenitizing and tempering (DTA) process resulted in a significant improvement of strength and toughness by refinement of prior austenite grains. In this study, it was investigated that the mechanism of improving mechanical properties according to the change of microstructure by the second fully austenitizing temperature of the DAT process for low alloy steel required the structural integrity. Compared to conventional single austenitizing and tempering (SAT) process, the tensile elongation properties have improved about 5%, DBTTs have obtained result in reduction of about -65℃, and grain size has decreased by about 50% in the DAT process conditions. Grain refinement has crack propagation interference effect due to an increase of the grain boundaries and amount of energy absorption at low temperatures. The higher first austenitizing temperature in the DAT process, the more increase the spheroidized carbides and strengthening the effect of fine precipitates in the ferrite grain. The area ratio of the dimple in the transition area has increased by proportion to the effect of spheroidized carbides. This may the primary mechanisms that can improve low-temperature toughness and elongation while maintaining a similar hardness and strength.

Keywords: double austenitizing, Ductile Brittle transition temperature, grain refinement, heat treatment, low alloy steel, low-temperature toughness

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Authors: Bing–Jing Zhao, Chang-Kui Liu, Hong Wang, Min Hu

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Electron beam rapid manufacturing (EBRM) or Selective laser melting is an additive manufacturing process that uses 3D CAD data as a digital information source and energy in the form of a high-power laser beam or electron beam to create three-dimensional metal parts by fusing fine metallic powders together.Object:The present study was conducted to evaluate the mechanical properties ,the phase transformation,the corrosivity and the biocompatibility of Ti-6Al-4V by EBRM,SLM and forging technique.Method: Ti-6Al-4V alloy standard test pieces were manufactured by EBRM, SLM and forging technique according to AMS4999,GB/T228 and ISO 10993.The mechanical properties were analyzed by universal test machine. The phase transformation was analyzed by X-ray diffraction and scanning electron microscopy. The corrosivity was analyzed by electrochemical method. The biocompatibility was analyzed by co-culturing with mesenchymal stem cell and analyzed by scanning electron microscopy (SEM) and alkaline phosphatase assay (ALP) to evaluate cell adhesion and differentiation, respectively. Results: The mechanical properties, the phase transformation, the corrosivity and the biocompatibility of Ti-6Al-4V by EBRM、SLM were similar to forging and meet the mechanical property requirements of AMS4999 standard. a­phase microstructure for the EBM production contrast to the a’­phase microstructure of the SLM product. Mesenchymal stem cell adhesion and differentiation were well. Conclusion: The property of the Ti-6Al-4V alloy manufactured by EBRM and SLM technique can meet the medical standard from this study. But some further study should be proceeded in order to applying well in clinical practice.

Keywords: 3D printing, Electron Beam Rapid Manufacturing (EBRM), Selective Laser Melting (SLM), Computer Aided Design (CAD)

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Authors: Mitia Ramarosaona, Sylvie Castagnet, Damien Halm, Henri-Alexandre Cayzac, Nicolas Dufaure, Philippe Papin

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In light of the ongoing energy transition, 'Infrastructure developments' for hydrogen transportation and storage raise studies on the materials employed for hyperbaric vessels. Type IV tanks represent the most mature choice for gaseous hydrogen storage at high pressure – 70MPa. These tanks are made of a composite shell and an internal hydrogen-exposed polymer liner. High pressure conditions lead to severe mechanical loading requiring high resistance. Liner is in contact with hydrogen and undergoes compression – decompression cycles during system filling and emptying. Stresses induced by this loading, coupled with hydrogen diffusion, were found to cause microstructural changes and degradation of mechanical behaviour after decompression phase in some studies on HDPE. These phenomena are similar to those observed in elastomeric components like sealing rings, which can affect permeability and lead to their failure. They may lead to a hydrogen leak, compromising security and tightness of the tank. While these phenomena have been identified in elastomers, they remain less addressed in thermoplastics and consequences post-decompression damages on mechanical behaviour and to the best of author's knowledge was not studied either. Different additives are also included in liner formulation to improve its behaviour. This study aimed to better understand damage micro-mechanisms in PA11s exposed to hydrogen compression-decompression cycles and understand if additives influence their resistance. Samples of pure, plasticized and impact-modified PA11s are exposed to 1, 3 and 8 pressure cycles including hydrogen saturation at 70MPa followed by severe 15-second decompression. After hydrogen exposure and significantly later than full desorption, the residual mechanical behaviour is characterized through impact and monotonic tensile tests, on plain and notched samples. Several techniques of microstructure and micro-nano damage characterization are carried out to assess whether changes in macroscopic properties are driven by microstructural changes in the crystalline structure (SAXS-WAXS acquisitions and SEM micrographs). Thanks to WAXS acquisition and microscopic observation, the effects due to additives and pressure consequences can be decorrelated. Pure PA11 and PA11 with a low percentage of additives show an increase in stress level at the first yielding point after hydrogen cycles. The amplitude of the stress increase is more important in formulation with additives because of changes in PA11 matrix behavior and environment created by additives actions. Plasticizer modifies chain mobility leading to microstructure changes while other additives, more ductile than PA11, is able to cavitate inside PA11 matrix when undergoing decompression. On plasticized formulation, plasticizer migration are suspected to enhance impact of hydrogen cycling on mechanical behaviour. Compared to the literature on HDPE and elastomers, no damages like cavitation or cracking could be evidenced from SAXS experiments on every PA11 formulation tested. In perspectives, on all formulation, experimental work is underway to confirm influence of residual pressure level after decompression on post-decompression damages level, the aim is to better understand the factors affecting the mechanical behavior of thermoplastics subject to mechanical solicitation from decompression in hydrogen tank liners, not mechanical behaviour of liner in hydrogen tanks directly.

Keywords: additives, hydrogen tank liner, microstructural analysis, PA11

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Authors: Hasan Kaya

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Effect of lead content on the microstructure, mechanical (microhardness, ultimate tensile strength) and electrical resistivity properties of Al–Si eutectic alloys has been investigated. Al–12.6 Si–xSn (x=1, 2, 4, 6 and 8 wt. %) were prepared using metals of 99.99% high purity in the vacuum atmosphere. These alloys were directionally solidified under constant temperature gradient (5.50 K/mm) and growth rate (8.25 μm/s) by using a Bridgman–type directional solidification furnace. Eutectic spacing, microhardness, ultimate tensile strength and electrical resistivity were expressed as functions of the composition by using a linear regression analysis. The dependency of the eutectic spacing, microhardness, tensile strength and electrical resistivity on the composition (Sn content) were determined. According to experimental results, the microhardness, ultimate tensile strength and electrical resistivity of the solidified samples increase with increasing the Sn content, but decrease eutectic spacing. Variation of electrical resistivity with the temperature in the range of 300-500 K for studied alloys was also measured by using a standard d.c. four-point probe technique.

Keywords: content elements, solidification, microhardness, strength

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Authors: Kristina Pflug, Markus Busch

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Being able to predict polymer properties and processing behavior based on the applied operating reaction conditions in one of the key challenges in modern polymer reaction engineering. Especially, for cost-intensive processes such as the high-pressure polymerization of low-density polyethylene (LDPE) with high safety-requirements, the need for simulation-based process optimization and product design is high. A multi-scale modelling approach was set-up and validated via a series of high-pressure mini-plant autoclave reactor experiments. The approach starts with the numerical modelling of the complex reaction network of the LDPE polymerization taking into consideration the actual reaction conditions. While this gives average product properties, the complex polymeric microstructure including random short- and long-chain branching is calculated via a hybrid Monte Carlo-approach. Finally, the processing behavior of LDPE -its melt flow behavior- is determined in dependence of the previously determined polymeric microstructure using the branch on branch algorithm for randomly branched polymer systems. All three steps of the multi-scale modelling approach can be independently validated against analytical data. A triple-detector GPC containing an IR, viscosimetry and multi-angle light scattering detector is applied. It serves to determine molecular weight distributions as well as chain-length dependent short- and long-chain branching frequencies. 13C-NMR measurements give average branching frequencies, and rheological measurements in shear and extension serve to characterize the polymeric flow behavior. The accordance of experimental and modelled results was found to be extraordinary, especially taking into consideration that the applied multi-scale modelling approach does not contain parameter fitting of the data. This validates the suggested approach and proves its universality at the same time. In the next step, the modelling approach can be applied to other reactor types, such as tubular reactors or industrial scale. Moreover, sensitivity analysis for systematically varying process conditions is easily feasible. The developed multi-scale modelling approach finally gives the opportunity to predict and design LDPE processing behavior simply based on process conditions such as feed streams and inlet temperatures and pressures.

Keywords: low-density polyethylene, multi-scale modelling, polymer properties, reaction engineering, rheology

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